CN100460003C

CN100460003C - Medicinal composition and its preparing method and quality control method

Info

Publication number: CN100460003C
Application number: CNB2005100552652A
Authority: CN
Inventors: 邹节明
Original assignee: Guilin Sanjin Pharmaceuticals Co Ltd
Current assignee: Guilin Sanjin Pharmaceuticals Co Ltd
Priority date: 2005-03-17
Filing date: 2005-03-17
Publication date: 2009-02-11
Anticipated expiration: 2025-03-17
Also published as: CN1682969A

Abstract

The present invention discloses medicine composition for treating women's inflammation and its preparation process and quality control method. The medicine composition contains flavescent sophora root, Chinese lizardtail herb, phellodendron bark, Cherokee rose root, corydalis tuber, etc. The medicine composition has the functions of clearing away heat and damp, stopping leukorrhagia and itching, dispersing blood clots, relieving pain, detoxicating and eliminating swelling, and is used to treat various women's inflammations. The present invention has determined curative effect and controllable quality.

Description

A kind of pharmaceutical composition and preparation method thereof and method of quality control

Invention field

The present invention relates to a kind of pharmaceutical composition and preparation method thereof and method of quality control, particularly a kind of pharmaceutical composition that is used for the treatment of gynecological inflammation and preparation method thereof and method of quality control.

Background technology

Chronic pelvic inflammatory disease comprises chronic endometritis, adnexitis, chronic salpingo-ocphoritis and chronic pelvic paramitritis, being the commonly encountered diseases and the frequently-occurring disease of department of obstetrics and gynecology, also is one of common cause that causes ectopic pregnancy, infertile, gynecological's pelvic pain and pelvic adhesion disease.Belong to Chinese medicine " leukorrheal diseases " category.Normal for acute pelvic inflammatory disease can not thoroughly treat or patient's body constitution relatively poor, due to the course of disease is delayed, but but also NAI medical history.The state of an illness is obstinate, when resistance is relatively poor, acute attack can be arranged.Because chronic pelvic inflammatory disease is shown effect repeatedly, delay is difficult, and how antibiotic has formed drug resistance, brings misery to the patient.

The chronic pelvic inflammatory disease sickness rate is on the rise at present.Spread unchecked country in some sexual openness, sexually transmitted disease (STD), this disease is particularly common.Estimate according to World Health Organization (WHO), sexually transmitted disease (STD) is spread unchecked and is caused annual newly-increased more than 300,000,000 3 thousand ten thousand std patients in the whole world, wherein have 10%～20% will develop into pelvic inflammatory disease, consequently bring a series of families and social problems such as long-term chronic pelvic pain, infertility or ectopic pregnancy.It is reported, 40% gynaecopathias of suffering from various degree such as reproductive tract infection in the Chinese women, married woman's prevalence is especially up to 70%.

Because the pathogeny to chronic pelvic inflammatory disease still lacks enough understandings at present, has every year thousands of patient to stay a series of sequela because of can not get in time treating completely.Chemicals is to this sick unsatisfactory curative effect, and Chinese medicine has advantages such as evident in efficacy, that side effect is little, relapse rate is low with this disease of the theoretical treatment of its unique determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs, is subjected to domestic and international medical expert's attention day by day.At present the report of clinical application Chinese medicine primary disease is more, has shown unique advantage and bright prospects that Chinese medicine should disease.

Comprehensively above-mentioned, chronic pelvic inflammatory disease sickness rate height is very big to patient's physical and mental health and family, social harm.Aspect this disease of treatment, chemicals unsatisfactory curative effect Chinese medicine then has special advantages and wide prospect.But the Chinese patent medicine that can effectively treat chronic pelvic inflammatory disease in the market is still not many, so the new Chinese medicine of the treatment chronic pelvic inflammatory disease of high effect nontoxic of research and development, taking convenience will produce high social and economic benefit.

Summary of the invention

One object of the present invention is to disclose a kind of pharmaceutical composition; Another object of the present invention is to disclose a kind of pharmaceutical composition that is used for the treatment of gynecological inflammation; The 3rd purpose of the present invention is to disclose a kind of preparation of drug combination method; The object of the invention also is to disclose a kind of method of quality control of pharmaceutical composition.

The crude drug of pharmaceutical composition of the present invention is formed and proportioning following (by weight):

Radix Picriae felterrae 10-95 weight portion Rhizoma Saururi (Herba Saururi) 10-80 weight portion Cortex Phellodendri 10-85 weight portion

Radix Rosae Laevigatae 50-200 weight portion Rhizoma Corydalis 10-60 weight portion.

It is (by weight) that the crude drug of pharmaceutical composition of the present invention is formed optimum ratio:

Radix Picriae felterrae 85 weight portion Rhizoma Saururi (Herba Saururi)s 15 weight portion Cortex Phellodendris 80 weight portions

Radix Rosae Laevigatae 60 weight portion Rhizoma Corydalis 50 weight portions.

Can also add on above basis: Rhizoma Smilacis Chinensis 50-200 weight portion is or/and Radix Angelicae Sinensis 10-80 weight portion.

Radix Rosae Laevigatae 60 weight portion Rhizoma Smilacis Chinensiss, 180 weight portions are or/and Radix Angelicae Sinensis 20 weight portions

Rhizoma Corydalis 50 weight portions.

Radix Picriae felterrae 20 weight portion Rhizoma Saururi (Herba Saururi)s 70 weight portion Cortex Phellodendris 20 weight portions

Radix Rosae Laevigatae 180 weight portion Rhizoma Smilacis Chinensiss, 70 weight portions are or/and Radix Angelicae Sinensis 70 weight portions

Rhizoma Corydalis 15 weight portions.

Radix Picriae felterrae 60 weight portion Rhizoma Saururi (Herba Saururi)s 40 weight portion Cortex Phellodendris 40 weight portions

Radix Rosae Laevigatae 140 weight portion Rhizoma Smilacis Chinensiss, 100 weight portions are or/and Radix Angelicae Sinensis 40 weight portions

Rhizoma Corydalis 27 weight portions.

Preparation of drug combination method of the present invention:

Radix Picriae felterrae adds 4-12 times of water gaging and decocts 2-3 time, and each 0.5～2 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.1-0.3 parts by volume water elution, discard eluent, use 35～75% 0.2 parts by volume ethanol and 0.03-0.1 part by volume water elution more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.06～1.40 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1-2 hour, collecting decoction, be concentrated into relative density and be 1.06～1.40 clear paste, add 75-99% ethanol and make the alcohol amount of containing reach 50-70%, fully stir, left standstill 2-4 hour, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.06～1.40 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 4～12 times of amount 0.2-0.5%, decoct 2-3 time, each 0.5-2 hour, collecting decoction was concentrated into relative density and is 1.01～1.10 extractum, add the sodium chloride that is equivalent to extractum amount 12-18%, stir evenly, leave standstill, centrifugal, precipitate adds 1-3 times of water gaging to be washed, centrifugal, drying precipitate is ground into fine powder, gets this pharmaceutical composition, this pharmaceutical composition can be made into clinical acceptable forms, comprises tablet, granule, capsule, oral liquid, drop pill etc.

Preparation of drug combination method of the present invention can also be: Radix Picriae felterrae adds 4-12 times of water gaging and decocts 2-3 time, and each 0.5～2 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.1-0.3 parts by volume water elution, discard eluent, use 35～75% 0.2 parts by volume ethanol and 0.03-0.1 parts by volume water elution more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.06～1.40 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Smilacis Chinensis and/or Radix Angelicae Sinensis, Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1-2 hour, collecting decoction, be concentrated into relative density and be 1.06～1.40 clear paste, add 75-99% ethanol and make the alcohol amount of containing reach 50-70%, fully stir, left standstill 2-4 hour, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.06～1.40 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 4～12 times of amount 0.2-0.5%, decoct 2-3 time, each 0.5-2 hour, collecting decoction was concentrated into relative density and is 1.01～1.10 extractum, add the sodium chloride that is equivalent to extractum amount 12-18%, stir evenly, leave standstill, centrifugal, precipitate adds 1-3 times of water gaging to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition can be made into tablet, granule, capsule, oral liquid or drop pill.

The w/v of above-mentioned raw materials used medicine and eluent is g/L.

The method of quality control of this composite preparation contains following discriminating and/or assay, and discrimination method is selected from one or more in the following method:

A. get 2.22 times of amounts of this pharmaceutical composition day taking dose, porphyrize adds methanol 20ml supersound process 20-40 minute, filters, and gets filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 15-30 minute, filter, filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution with the 10-15:4-8:2-4:2-4:1-2 ratio is developing solvent, with developing solvent and strong ammonia solution pre-equilibration 12-18 minute simultaneously, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

B. get the filtrate under a item, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 20-40 minute, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 8-12:4-6:1-2 ratio is developing solvent, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

C. get the sodium carbonate liquid under the b item, fling to remaining ether, use ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, supersound process 20-40 minute, filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 15-18:2-5 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

Content assaying method is:

With octadecylsilane chemically bonded silica is filler; 35-40:60-65:0.4-0.6 the acetonitrile-water-glacial acetic acid of ratio is a mobile phase; The detection wavelength is 264nm; Number of theoretical plate calculates by Radix Picriae felterrae glycosides IA peak should be not less than 5000;

It is an amount of that precision takes by weighing Radix Picriae felterrae glycosides IA reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Get 2.22 times of amounts of this pharmaceutical composition day taking dose, the accurate title, decided porphyrize, get about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 40-50 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, promptly; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate, and take amount of formulation this pharmaceutical composition day and contain Radix Picriae felterrae with Radix Picriae felterrae glycosides IA (C ₄₁H ₆₂O ₁₃) meter, must not be less than 4.68mg.

This pharmaceutical composition day, the taking dose phase took crude drug amount 40.23 grams the same day.

The present invention has that heat clearing and damp drying, leukorrhagia stopping are antipruritic, the effect of eliminating stasis to stop pain, removing toxic substances and promoting subsidence of swelling.The symptom of the disease of being treated mainly shows: profuse leukorrhea, and yellow skin matter is thick, or color Semen Vignae Cylindricae slag specimen, pruritus vulvae, lower abdominal distention pain, the bitter taste greasy taste in the mouth, uncomfortable in chest indigestion and loss of appetite, oliguria with reddish urine, red tongue with yellowish and greasy fur, slippery and rapid pulse etc.; Chronic pelvic inflammatory disease is seen above-mentioned patient.The preparation stabilization that the present invention realizes, quality controllable.

Pharmacodynamics to the pharmaceutical composition tablet (temporarily name three gold medal woman scorching sheet) of these seven flavors crude drug partly carries out preliminary study, and the result shows: this pharmaceutical composition has antiinflammatory, analgesic, itching relieving effect; Thermostimulation there is analgesic activity, but chemical stimulation is not had analgesic activity; Inhibited to antibacterials such as staphylococcus aureus, pouring ball Neisseria, escherichia coli, group B streptococcus and Pseudomonas aeruginosas, aseptic and bacillary gynecological inflammation all there are significant inhibitory effect; Has the expansion blood capillary, the effect of microcirculation improvement.Following experimental example is used to further specify the present invention:

Experimental example 1: antiinflammatory test

The scorching test of Mice Auricle caused by dimethylbenzene xylene: get 75 of mices, be divided into 6 groups at random, at least 10 every group, be administered once every day, and matched group is given the equal-volume normal saline, and gastric infusion is 5 days continuously.1h the two sides evenly is coated with dimethylbenzene 0.02ml before and after every Mus auris dextra with polishing 4 (1/2) numbers syringe needles after the last administration.With sacrifice of animal, the mice ears are downcut scales/electronic balance weighing with the position homalographic after 15 minutes with diameter 8mm card punch.Every Mus auris dextra sheet weight deducts left auricle weight and calculates the swelling degree.

Swelling degree=auris dextra sheet weight-left auricle weight

The result: the swelling degree of ear swelling has been compared reduction with matched group due to the basic, normal, high dosage group of the scorching sheet of three gold medal woman and the aspirin group xylol, and difference has significance (P＜0.05, P＜0.01).Point out the scorching sheet of three gold medal woman that antiinflammatory action is arranged.

Experimental example 2: analgesic test

Conventional hot plate method test: before the test mice is screened, be placed on 55+1 ℃ the hot plate, lick metapedes required time (s) and be the normal pain threshold of this Mus to mice occurring with the placement hot plate.All persons that just occurs licking the metapedes in 5s or behind 30s and leaper all give it up.Select 90 of qualified mices, be divided into 6 groups at random.Qualified mice is fasting 12h before test, for drinking-water.The normal pain threshold of each Mus of replication. by each group dosage gastric infusion, matched group is given the equal-volume normal saline then, respectively at after the administration 15,30,60 and 120min measure the pain threshold of respectively organizing mice respectively.Mice stops on hot plate and surpasses still nonresponder of 60s, and calculate with 60s its threshold of pain.Calculate the percentage rate (%) that improve the threshold of pain behind the medicine as follows:

Average pain threshold * 100% before the percentage rate that improve the threshold of pain=(the preceding average pain threshold of average pain threshold-medication after the medication)/medication

Result: compare with matched group, the scorching sheet high dose group of three gold medal woman threshold value of 15 and 30 minutes after administration raises, difference has significance meaning (P＜0.05), simultaneously aspirin group threshold value of 60 and 120 minutes after administration raises, difference has significance meaning (P＜0.05), and other group does not have the significance meaning.Prompting this product is to ease pain by central analgesia rather than by periphery to bring into play its pharmacological action.

Experimental example 3: separate heat test

Get 36 of new zealand white rabbits, every animal body temperature every day fluctuation is no more than 0.4 ℃, respectively surveys one time body temperature, continuous two days after the purchase again every day in morning and afternoon.Ear vein injection endotoxin (24EU/Kg) modeling type after surveying body temperature in the 3rd day was surveyed body temperature after 1 hour, was divided into 6 groups at random by body temperature, listed medicine and dosage gastric infusion, and matched group gives isopyknic soybean salad oil.Surveyed a body temperature later on every 1 hour.The difference (being lift-off value) of body temperature that each time point records and basal body temperature (average of the first five time of moulding body temperature) compares with matched group, carries out statistical procedures with the t check, and is abscissa with time, and the fervescence value is the vertical coordinate time of drawing-anus temperature curve.

Result of the test: compare with matched group, the temperature of the scorching sheet high dose group of three gold medal woman of 3 hours and 4 hours reduces after the administration significant difference (P＜0.05), after the administration in the scorching sheet of 4,5 and 6 hours three gold medal woman the temperature of dosage group reduce significant difference (P＜0.05) arranged, and the temperature reduction of 3 hours and 4 hours after administration of the scorching sheet of three gold medal woman is dose dependent, the aspirin group reduces 2,3,4,5 and 6 hours group temperature significant difference (P＜0.05), but the JINJI PIAN group is at each time point there was no significant difference (P〉0.05) all.Prompting the present invention has refrigeration function.

Experimental example 4: antipruritic test

Get 50 of Cavia porcelluss, divide 5 groups at random, 10 every group, establish normal control group, positive group, high, medium and low three the dosage groups of the medicine that is put to the test, matched group is given the equal-volume normal saline, and gastric infusion is 5 days continuously.The test proxima luce (prox. luc) to each the right back instep of group Cavia porcellus unhairing, is tested the same day, abrades unhairing place, right back instep with rough sand paper, and area is 1cm ², be administered once.1h after the last medication, beginning is only dripped 0.01% 0.05ml/ of histamine phosphate at wound surface, after this complies with 0.01%, 0.02%, 0.03%, 0.04% every 3 minutes---and progressive concentration, each 0.05ml/ is only.Directly causing the histamine phosphate's total amount that gives when Cavia porcellus occurs later licking metapedes is itch-threshold.

The result: compare with matched group, scorching basic, normal, high dosage group of sheet of three gold medal woman and diphenhydramine group have the effect of rising itch-threshold, and difference has significance meaning (P＜0.05).Prompting this product has itching-relieving action.

Experimental example 5: in-vitro antibacterial test

The agar dilution of recommending according to U.S. clinical laboratory standardization committee (NCCLS) carries out ^[1]Concrete grammar is as follows: take by weighing this Chinese medicine of 10g, add sterile distilled water 15ml, make the medicine suspension of 666mg/ml (W/V) after stirring, successively it is diluted with aseptic agar culture medium respectively again, make the test agar flat board that contains 66.6mg/ml, 33.3mg/ml, 16.65mg/ml, 8.3mg/ml, 4.2mg/ml medicine respectively.Each test organisms (aspergillus niger spore) dilutes with normal saline earlier and proofreaies and correct to 0.5 Maxwell unit (bacteria concentration about 10 ⁸CFU/mL), respectively organize the test agar flat board then and inoculate corresponding test organisms respectively, each plating bacterium amount is about 10 ⁴Individual antibacterial.Cultivate 18-24 hour observed result for 37 ℃, judge minimal inhibitory concentration (MIC).Each corresponding dilution medicinal liquid with the agar culture medium dilution does not add antibacterial, contrasts as medicine; Positive control is to add identical bacterium amount but the agar culture medium that do not add medicinal liquid; Negative control is not for adding the agar culture medium of antibacterial.

The result: the scorching sheet of three gold medal woman is 8.3mg/ml to staphylococcus aureus, Diplococcus gonorrhoeae minimal inhibitory concentration (MIC), MIC to escherichia coli is 33.3mg/ml, MIC to group B streptococcus and Pseudomonas aeruginosa is 66.6mg/ml, and to the MIC of fungus such as candida albicans bacterium and aspergillus niger all greater than 66.6mg/ml.Prompting this product has antibacterial action.

Experimental example 6: chronic endometritis test

Get 70 not female rats of copulation, 10% chloral hydrate 0.3ml/100g anesthesia, routine disinfection, hypogastric region down in the about 2cm of otch, the exposure uterus, with No. 4 syringe needles respectively at the careful inserting needle of uterus crotch, slowly inject 25% phenol rubber cement 0.04ml to the ovary direction, injection finishes, and abdomen is closed in layering, sterilization.Wherein 10 rats are not injected phenol as sham operated rats.The treatment of postoperative beginning on the seven gastric infusion, the dosage volume is 1.0ml/100g, dosage sees Table 20-7.After 4 weeks of medication, 1h after the last administration gets the hematometry peripheral blood leucocyte, puts to death, and perusal is also write down the uterus and changed substantially, wins the uterus, left side, and the back of weighing is fixed with neutral formalin, conventional section, and HE dyeing is carried out pathological examination, semi-quantitative analysis.

Swelling rate (%)=(uterus, weight-right side, uterus, left side is heavy)/uterus, right side is heavy; Suppression ratio (%)=(model control group swelling rate-each medicine group swelling rate)/model control group swelling rate

The result: compare with sham operated rats, the leukocyte count of scorching each the dosage group of sheet of three gold medal woman is the reduction of dose dependent; The uterus swelling rate of scorching sheet high dose group of three gold medal woman and aspirin group all obviously reduces, difference has significance meaning (being respectively P＜0.05 and P＜0.01), pathological examination shows, compare with model control group, aspirin and high dose group intra-uterine membranous layer and flesh layer are all seen a small amount of eosinophil leucocyte and lymphocytic infiltration, dosage and JINJI PIAN group intra-uterine membranous layer and flesh layer are all seen more amount eosinophil leucocyte and lymphocytic infiltration simultaneously, and low dose group intra-uterine membranous layer and flesh layer are all seen volume eosinophil leucocyte and lymphocytic infiltration.Prompting the present invention has the effect that suppresses the aseptic endometrial inflammation.

Experimental example 7: chronic pelvic inflammatory disease test

Get 70 not female rats of copulation, 10% chloral hydrate 0.3ml/100g anesthesia, routine disinfection, the down middle about 2cm of otch of hypogastric region exposes the uterus, and respectively at the careful inserting needle of uterus crotch, the ovary direction is slowly injected bacterium liquid (10 to the left with No. 4 syringe needles ⁶～10 ⁷/ ml0.08ml), injection finishes, and abdomen is closed in layering, sterilization.Wherein 10 rats are not injected bacterium liquid as sham operated rats.The treatment of postoperative beginning on the seven gastric infusion, the dosage volume is 1.0ml/100g.After 4 weeks of medication, 1h after the last administration gets the hematometry peripheral blood leucocyte, puts to death, and perusal is also write down the uterus and changed substantially, wins the uterus, left side, and the back of weighing is fixed with neutral formalin, conventional section, and HE dyeing is carried out pathological examination, semi-quantitative analysis.

The result: compare with sham operated rats, the leukocyte count of scorching each the dosage group of sheet of three gold medal woman is the reduction of dose dependent; Scorching middle and high dosage group of sheet of three gold medal woman and amoxicillin group all obviously reduce, and difference has significance meaning (being respectively P＜0.05 and P＜0.01).Pathological examination shows, compare with model control group, aspirin and high dose group intra-uterine membranous layer and flesh layer are all seen a small amount of eosinophil leucocyte and lymphocytic infiltration, dosage and JINJI PIAN group intra-uterine membranous layer and flesh layer are all seen more amount eosinophil leucocyte and lymphocytic infiltration simultaneously, and low dose group intra-uterine membranous layer and flesh layer are all seen volume eosinophil leucocyte and lymphocytic infiltration.Prompting this product has the effect of anti-caused by Staphylococcus aureus pelvic inflammation.

Experimental example 8: microcirculation test

Get 60 of healthy kunming mices, be divided into six groups at random, i.e. normal saline group, the aspirin group, the scorching sheet of compound Salviae Miltiorrhizae group and three gold medal woman low, in, high dose group.Aspirin group 0.225g/kg wherein, FUFANG DANSHEN PIAN 0.42g/kg, the scorching sheet of three gold medal woman low, in, high dose is respectively 0.2g/kg, 0.4g/kg and 0.8g/kg.The amount 0.3ml that the normal saline group gives equal volume irritates stomach.Every group 10, weigh and random number.Mice with after the urethane anesthesia, is faced upward the position with mice and is fixed in the mouse ear holder, regulate the height of measuring platform on the microscope, make auricle open and flat in the ear holder.Be coated with a little cedar oil at auricle, the auricle back side, regulate the suitable brightness of cold light source, under transillumination, choosing suitable position observation is moving down with 50～100 power microscopes, vein blood vessel bore, the open number of blood capillary, blood fluidised form and flow velocity, the labelling look-out station, gastric infusion, 15min after the observation administration, 30min, observe the same position of Mice Auricle artery and vein external caliber, the open number of blood capillary, blood fluidised form and flow velocity in same times behind 45min and the 60min.Carry out dynamic analysis with camera system and medical images analytical system simultaneously.

The result: after the administration 15,30,45,60 minutes, the vein of the high and middle dosage group of the scorching sheet of three gold medal woman with the increase of tremulous pulse bore, the venous blood flow velocity variations is compared with matched group that significant difference (p＜0.01) is all arranged; After the administration 30,45,60 minutes, the open number of the scorching sheet of three gold medal woman blood capillary high and middle dosage group, venous blood fluidised form mark to compare with matched group all had significant difference (p＜0.01); After the administration 30,45,60 minutes, the vein of the scorching sheet low dose group of three gold medal woman with tremulous pulse bore, the open number of blood capillary, venous blood flow velocity variations, the scoring of venous blood fluidised form is compared with matched group all has significance to increase (p＜0.05, p＜0.01).Show that this product has the expansion blood capillary, the effect of microcirculation improvement.

Embodiment 1:

Radix Picriae felterrae 60g Rhizoma Saururi (Herba Saururi) 40g Cortex Phellodendri 40g Radix Rosae Laevigatae 140g Rhizoma Corydalis 27g

Radix Picriae felterrae adds 8 times of water gagings and decocts secondary, each 1 hour, collecting decoction, centrifugal, filtrate is used the 0.2L water elution by styrene tyle macroporous adsorption resin, discard eluent, use 50% ethanol 0.2L and water 0.05L eluting more successively, merge eluent, reclaim ethanol, being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Corydalis (vinegar system) and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, being concentrated into relative density is the clear paste of 1.12～1.16 (60 ℃), add 85% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, and being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 8 times of amounts 0.3%, decoct secondary, each 1 hour, collecting decoction, being concentrated into relative density is the extractum of 1.02～1.04 (60 ℃), adds the sodium chloride that is equivalent to extractum amount 15%, stirs evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings to be washed, centrifugal, drying precipitate is ground into fine powder, adds an amount of starch, mixing is made granule, adds carboxymethyl starch sodium, Pulvis Talci and magnesium stearate mixing, be pressed into tablet, the bag film-coat, promptly.The heavy 0.24g of every in made tablet, one time 3, every day 3 times.

Embodiment 2:

Radix Picriae felterrae 85g Rhizoma Saururi (Herba Saururi) 15g Cortex Phellodendri 80g Radix Rosae Laevigatae 60g

Rhizoma Smilacis Chinensis 180g Radix Angelicae Sinensis 20g Rhizoma Corydalis 50g

Radix Picriae felterrae adds 5 times of water gagings and decocts secondary, and 0.5 hour for the first time, 1.5 hours for the second time, collecting decoction, centrifugal, filtrate is passed through styrene tyle macroporous adsorption resin, use the 0.15L water elution, discard eluent, use 40% ethanol 0.2L and water 0.04L eluting more successively, merge eluent, reclaim ethanol, being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), drying, be ground into fine powder, standby; Get Radix Rosae Laevigatae, Rhizoma Smilacis Chinensis, Rhizoma Saururi (Herba Saururi), Radix Angelicae Sinensis, Rhizoma Corydalis (vinegar system) and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, being concentrated into relative density is the clear paste of 1.12～1.16 (60 ℃), add 90% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 2 hours, centrifugal, supernatant reclaims ethanol, and being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 5 times of amounts 0.3%, decoct secondary, each 1 hour, collecting decoction, being concentrated into relative density is the extractum of 1.02～1.04 (60 ℃), add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings and washes, centrifugal, drying precipitate is ground into fine powder.Add an amount of starch, mixing is made granule.The heavy 5g of every bag of made granule, one time 2 bags, every day 3 times.

Embodiment 3:

Radix Picriae felterrae 20g Rhizoma Saururi (Herba Saururi) 70g Cortex Phellodendri 20g Radix Rosae Laevigatae 180g Rhizoma Corydalis 15g

Radix Picriae felterrae adds 10 times of water gagings and decocts secondary, each 1.5 hours, collecting decoction, centrifugal, filtrate is used the 0.2L water elution by styrene tyle macroporous adsorption resin, discard eluent, use 70% ethanol 0.2L and water 0.08L eluting more successively, merge eluent, reclaim ethanol, being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Corydalis (vinegar system) and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, being concentrated into relative density is the clear paste of 1.12～1.16 (60 ℃), add 95% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, and being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 10 times of amounts 0.3%, decoct secondary, each 1.5 hours, collecting decoction, being concentrated into relative density is the extractum of 1.02～1.04 (60 ℃), add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings and washes, centrifugal, drying precipitate is ground into fine powder.Make capsule.The heavy 0.5g of every of made capsule, one time 3, every day 3 times.

Embodiment 4:

Embodiment 5:

Embodiment 6:

Radix Picriae felterrae 20g Rhizoma Saururi (Herba Saururi) 70g Cortex Phellodendri 20g Radix Rosae Laevigatae 180g

Rhizoma Smilacis Chinensis 70g Radix Angelicae Sinensis 70g Rhizoma Corydalis 15g

Radix Picriae felterrae adds 10 times of water gagings and decocts secondary, each 1.5 hours, collecting decoction, centrifugal, filtrate is used the 0.2L water elution by styrene tyle macroporous adsorption resin, discard eluent, use 70% ethanol 0.2L and water 0.08L eluting more successively, merge eluent, reclaim ethanol, being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Smilacis Chinensis, Rhizoma Saururi (Herba Saururi), Radix Angelicae Sinensis, Rhizoma Corydalis (vinegar system) and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, being concentrated into relative density is the clear paste of 1.12～1.16 (60 ℃), add 95% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, and being concentrated into relative density is the clear paste of 1.14～1.18 (60 ℃), spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 10 times of amounts 0.3%, decoct secondary, each 1.5 hours, collecting decoction, being concentrated into relative density is the extractum of 1.02～1.04 (60 ℃), add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings and washes, centrifugal, drying precipitate is ground into fine powder.Make capsule.The heavy 0.5g of every of made capsule, one time 3, every day 3 times.

Embodiment 7:

Radix Picriae felterrae 85g Rhizoma Saururi (Herba Saururi) 15g Cortex Phellodendri 80g

Radix Rosae Laevigatae 60g Rhizoma Smilacis Chinensis 180g Rhizoma Corydalis 50g

Common process is made capsule.The heavy 0.5g of every of made capsule, one time 3, every day 3 times.

Embodiment 8:

Radix Picriae felterrae 20g Rhizoma Saururi (Herba Saururi) 70g Cortex Phellodendri 20g

Radix Rosae Laevigatae 180g Rhizoma Smilacis Chinensis 70g Rhizoma Corydalis 15g

Common process is made granule, every bag heavy 5g, one time 2 bags, every day 3 times.

Embodiment 9:

Radix Picriae felterrae 60g Rhizoma Saururi (Herba Saururi) 40g Cortex Phellodendri 40g

Radix Rosae Laevigatae 140g Rhizoma Smilacis Chinensis 100g Rhizoma Corydalis 27g

Common process is made tablet, every heavy 0.24g, one time 3, every day 3 times.

Embodiment 10:

Radix Rosae Laevigatae 60g Radix Angelicae Sinensis 20g Rhizoma Corydalis 50g

Embodiment 11:

Radix Rosae Laevigatae 180g Radix Angelicae Sinensis 70g Rhizoma Corydalis 15g

Embodiment 12:

Radix Rosae Laevigatae 140g Radix Angelicae Sinensis 40g Rhizoma Corydalis 27g

Embodiment 13:The discrimination method of this composition tablet:

Get 20 in this pharmaceutical composition tablet, porphyrize adds methanol 20ml supersound process 30 minutes, filters, and gets filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with the benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution of 12:6:3:3:1 ratio, with developing solvent and strong ammonia solution while pre-equilibration 15 minutes, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

Embodiment 14:The discrimination method of this compositions:

A. get the filtrate of embodiment 4, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 30 minutes, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 10:5:1 ratio is developing solvent, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

B. the sodium carbonate liquid under the present embodiment a item is flung to remaining ether, uses ethyl acetate extraction 2 times, and each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, and supersound process 30 minutes filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 17:3 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

Embodiment 15:The discrimination method of this composition capsule:

A. get 20 of this medicament composition capsule agent, porphyrize adds methanol 20ml supersound process 30 minutes, filters, and gets filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with the benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution of 12:6:3:3:1 ratio, with developing solvent and strong ammonia solution while pre-equilibration 15 minutes, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

B. get the filtrate under the present embodiment a item, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 30 minutes, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 10:5:1 ratio is developing solvent, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

C. get the sodium carbonate liquid under the present embodiment b item, fling to remaining ether, use ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, and supersound process 30 minutes filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 17:3 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

Embodiment 16:The content assaying method of this composition tablet:

With octadecylsilane chemically bonded silica is filler; 38:62:0.5 the acetonitrile-water-glacial acetic acid of ratio is a mobile phase; The detection wavelength is 264nm; Number of theoretical plate calculates by Radix Picriae felterrae glycosides IA peak should be not less than 5000;

It is an amount of that precision takes by weighing Radix Picriae felterrae glycosides IA reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Get among the embodiment 1 20 of this pharmaceutical compositions, accurate claim fixed, porphyrize, get about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 45 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, promptly; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate, and every in this pharmaceutical composition tablet contains Radix Picriae felterrae with Radix Picriae felterrae glycosides IA (C ₄₁H ₆₂O ₁₃) meter, must not be less than 0.52mg.

Embodiment 17:The method of quality control of this composition tablet:

Discrimination method:

A. get 20 in this pharmaceutical composition tablet, porphyrize adds methanol 20ml supersound process 30 minutes, filters, and gets filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with the benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution of 12:6:3:3:1 ratio, with developing solvent and strong ammonia solution while pre-equilibration 15 minutes, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

B. get the filtrate under a item, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 30 minutes, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 10:5:1 ratio is developing solvent, launch, take out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

C. get the sodium carbonate liquid under the b item, fling to remaining ether, use ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, and supersound process 30 minutes filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 17:3 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

Content assaying method is:

With octadecylsilane chemically bonded silica is filler; 38:62:0.5 the acetonitrile-water-glacial acetic acid of ratio is a mobile phase; The detection wavelength is 264nm; Number of theoretical plate calculates by Radix Picriae felterrae glycosides IA peak should be not less than 5000; It is an amount of that precision takes by weighing Radix Picriae felterrae glycosides IA reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Get among the embodiment 1 20 of this pharmaceutical compositions, accurate claim fixed, porphyrize, get about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 45 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, promptly; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate, and every in this pharmaceutical composition tablet contains Radix Picriae felterrae with Radix Picriae felterrae glycosides IA (C ₄₁H ₆₂O ₁₃) meter, must not be less than 0.52mg.

Claims

1. pharmaceutical composition for the treatment of chronic pelvic inflammatory disease, the crude drug that it is characterized in that this pharmaceutical composition forms and weight proportion is:

Radix Picriae felterrae 10-95 weight portion Rhizoma Saururi (Herba Saururi) 10-80 weight portion Radix Rosae Laevigatae 50-200 weight portion

Cortex Phellodendri 10-85 weight portion Rhizoma Corydalis 10-60 weight portion.

2. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug composition and the weight proportion of this pharmaceutical composition is:

Radix Rosae Laevigatae 60 weight portion Rhizoma Corydalis 50 weight portions.

3. pharmaceutical composition as claimed in claim 1 or 2, it is characterized in that the crude drug composition of this pharmaceutical composition is added: Rhizoma Smilacis Chinensis 50-200 weight portion is or/and Radix Angelicae Sinensis 10-80 weight portion.

4. pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug composition and the weight proportion of this pharmaceutical composition is:

Radix Rosae Laevigatae 60 weight portion Rhizoma Corydalis 50 weight portions

Rhizoma Smilacis Chinensis 180 weight portions are or/and Radix Angelicae Sinensis 20 weight portions.

5. pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug composition and the weight proportion of this pharmaceutical composition is:

Radix Rosae Laevigatae 180 weight portion Rhizoma Corydalis 15 weight portions

Rhizoma Smilacis Chinensis 70 weight portions are or/and Radix Angelicae Sinensis 70 weight portions.

6. pharmaceutical composition as claimed in claim 3 is characterized in that the crude drug composition and the weight proportion of this pharmaceutical composition is:

Radix Rosae Laevigatae 140 weight portion Rhizoma Corydalis 27 weight portions

Rhizoma Smilacis Chinensis 100 weight portions are or/and Radix Angelicae Sinensis 40 weight portions.

7. preparation of drug combination method as claimed in claim 1 or 2 is characterized in that this method is:

Radix Picriae felterrae adds 4-12 times of water gagings and decocts 2-3 times, and each 0.5～2 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.1-0.3 parts by volume water elution, discard eluent, use 35～75% ethanol and 0.03-0.1 parts by volume water elution of 0.1 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.06～1.40 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1-2 hour, collecting decoction, be concentrated into relative density and be 1.06～1.40 clear paste, add 75-99% ethanol and make and contain alcohol amount and reach 50-70%, fully stir, left standstill 2-4 hours, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.06～1.40 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 4～12 times of amounts 0.2-0.5%, decoct 2-3 time, each 0.5-2 hours, collecting decoction was concentrated into relative density and is 1.01～1.10 extractum, add the sodium chloride that is equivalent to extractum amount 12-18%, stir evenly, leave standstill, centrifugal, precipitate adds 1-3 times of water gaging to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or drop pill.

8. preparation of drug combination method as claimed in claim 7 is characterized in that this method is:

Radix Picriae felterrae adds 8 times of water gagings and decocts secondary, each 1 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.2 parts by volume water elution, discard eluent, use 50% ethanol and the 0.05 parts by volume water elution of 0.2 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.14～1.18 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, be concentrated into relative density and be 1.12～1.16 clear paste, add 85% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.14～1.18 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 8 times of amounts 0.3%, decoct secondary, each 1 hour, collecting decoction was concentrated into relative density and is 1.02～1.04 extractum, add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or drop pill.

9. preparation of drug combination method as claimed in claim 3 is characterized in that this method is:

Radix Picriae felterrae adds 4-12 times of water gaging and decocts 2-3 time, and each 0.5～2 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.1-0.3 parts by volume water elution, discard eluent, use 35～75% ethanol and the 0.03-0.1 parts by volume water elution of 0.2 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.06～1.40 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Smilacis Chinensis or/and Radix Angelicae Sinensis, Rhizoma Corydalis add 4 times of water gagings and decoct twice, each 1-2 hour, collecting decoction, be concentrated into relative density and be 1.06～1.40 clear paste, add 75-99% ethanol and make the alcohol amount of containing reach 50-70%, fully stir, left standstill 2-4 hour, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.06～1.40 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 4～12 times of amount 0.2-0.5%, decoct 2-3 time, each 0.5-2 hour, collecting decoction was concentrated into relative density and is 1.01～1.10 extractum, add the sodium chloride that is equivalent to extractum amount 12-18%, stir evenly, leave standstill, centrifugal, precipitate adds 1-3 times of water gaging to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or drop pill.

10. preparation of drug combination method as claimed in claim 9 is characterized in that this method is:

Radix Picriae felterrae adds 8 times of water gagings and decocts secondary, each 1 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 2 parts by volume water elutions, discard eluent, use 50% ethanol and the 0.05 parts by volume water elution of 0.2 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.14～1.18 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Saururi (Herba Saururi), Rhizoma Smilacis Chinensis or/and Radix Angelicae Sinensis, Rhizoma Corydalis add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, be concentrated into relative density and be 1.12～1.16 clear paste, add 85% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.14～1.18 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 8 times of amounts 0.3%, decoct secondary, each 1 hour, collecting decoction was concentrated into relative density and is 1.02～1.04 extractum, add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or the drop pill of clinical acceptance.

11., it is characterized in that this method is as claim 4,5 or 6 described preparation of drug combination methods:

Radix Picriae felterrae adds 4-12 times of water gaging and decocts 2-3 time, and each 0.5～2 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.1-0.3 parts by volume water elution, discard eluent, use 35～75% ethanol and the 0.03-0.1 parts by volume water elution of 0.2 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.06～1.40 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Smilacis Chinensis, Rhizoma Saururi (Herba Saururi), Radix Angelicae Sinensis, Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1-2 hour, collecting decoction, be concentrated into relative density and be 1.06～1.40 clear paste, add 75-99% ethanol and make the alcohol amount of containing reach 50-70%, fully stir, left standstill 2-4 hour, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.06～1.40 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 4～12 times of amount 0.2-0.5%, decoct 2-3 time, each 0.5-2 hour, collecting decoction was concentrated into relative density and is 1.01～1.10 extractum, add the sodium chloride that is equivalent to extractum amount 12-18%, stir evenly, leave standstill, centrifugal, precipitate adds 1-3 times of water gaging to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or the drop pill of clinical acceptance.

12. preparation of drug combination method as claimed in claim 11 is characterized in that this method is:

Radix Picriae felterrae adds 8 times of water gagings and decocts secondary, each 1 hour, collecting decoction, centrifugal, filtrate is by styrene tyle macroporous adsorption resin, with 0.2 parts by volume water elution, discard eluent, use 50% ethanol and the 0.05 parts by volume water elution of 0.2 parts by volume more successively, merge eluent, reclaim ethanol, be concentrated into relative density and be 1.14～1.18 clear paste, drying is ground into fine powder, and is standby; Get Radix Rosae Laevigatae, Rhizoma Smilacis Chinensis, Rhizoma Saururi (Herba Saururi), Radix Angelicae Sinensis, Rhizoma Corydalis and add 4 times of water gagings and decoct twice, each 1 hour, collecting decoction, be concentrated into relative density and be 1.12～1.16 clear paste, add 85% ethanol and make and contain alcohol amount and reach 60%, fully stir, leave standstill more than 3 hours, centrifugal, supernatant reclaims ethanol, is concentrated into relative density and is 1.14～1.18 clear paste, spray drying, be ground into fine powder, standby; Get Cortex Phellodendri, add the sulfuric acid solution of 8 times of amounts 0.3%, decoct secondary, each 1 hour, collecting decoction was concentrated into relative density and is 1.02～1.04 extractum, add the sodium chloride that is equivalent to extractum amount 15%, stir evenly, leave standstill, centrifugal, precipitate adds 2 times of water gagings to be washed, centrifugal, drying precipitate, be ground into fine powder, get this pharmaceutical composition, this pharmaceutical composition is made tablet, granule, capsule, oral liquid or the drop pill of clinical acceptance.

13., it is characterized in that comprising in this method in the following discrimination method one or more as the method for quality control of claim 1,2,4,5 or 6 described pharmaceutical compositions:

A. get 2.22 times of amounts of this pharmaceutical composition day taking dose, add methanol 20ml supersound process 20-40 minute, filter, get filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 15-30 minute, filter, filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with the benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution of 10-15:4-8:2-4:2-4:1-2 ratio, with developing solvent and strong ammonia solution while pre-equilibration 12-18 minute, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

B. get the filtrate under a item, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 20-40 minute, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 8-12:4-6:1-2 ratio is developing solvent, launches, and takes out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

C. get the sodium carbonate liquid under the b item, fling to remaining ether, use ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, supersound process 20-40 minute, filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 15-18:2-5 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

14. method of quality control as claimed in claim 13 is characterized in that comprising in this method in the following discrimination method one or more:

A. get 2.22 times of amounts of this pharmaceutical composition day taking dose, add methanol 20ml supersound process 30 minutes, filter, get filtrate 1ml as need testing solution, all the other filtrate for later use; Other gets Cortex Phellodendri control medicinal material 0.1g, adds methanol 5ml, and supersound process 20 minutes filters, and filtrate is medical material solution in contrast; Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 2～4 μ l of need testing solution and control medicinal material solution, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with the benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution of 12:6:3:3:1 ratio, with developing solvent and strong ammonia solution while pre-equilibration 15 minutes, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

B. get the filtrate under a item, evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, and each 20ml merges ether solution, and evaporate to dryness, residue add methanol 1ml makes dissolving, and as need testing solution, sodium carbonate liquid is standby; Other gets Rhizoma Corydalis control medicinal material 0.5g, adds methanol 20ml supersound process 30 minutes, filters, and the filtrate evaporate to dryness shines medical material solution in pairs with legal system; Get the tetrahydropalmatine reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 15～20 μ l, control medicinal material solution 10 μ l, reference substance solution 2 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose that contains 1% sodium hydroxide solution, normal hexane-chloroform-methanol with the 10:5:1 ratio is developing solvent, launches, and takes out, dry, smoked clear with iodine vapor to the speckle colour developing, in air, wave the iodine that adsorbs on the most plate after, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

C. get the sodium carbonate liquid under the b item, fling to remaining ether, use ethyl acetate extraction 2 times, each 20ml merges ethyl acetate liquid, and evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Rosae Laevigatae control medicinal material 2g, adds methanol 20ml, and supersound process 30 minutes filters, filtrate evaporate to dryness, residue add 1% sodium carbonate liquor 20ml, and slight fever makes dissolving, use ether extraction 2 times, each 20ml discards ether solution, divides and gets sodium carbonate liquid, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10～15 μ l of need testing solution and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol with the 17:3 ratio is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of an above same color.

15., it is characterized in that comprising in this method following content assaying method as the method for quality control of claim 1,2,4,5 or 6 described pharmaceutical compositions:

It is an amount of that precision takes by weighing Radix Picriae felterrae glycosides IA reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Get 2.22 times of amounts of this pharmaceutical composition day taking dose, the accurate title, decided porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 40-50 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, promptly; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate, and take amount of formulation this pharmaceutical composition day and contain Radix Picriae felterrae in Radix Picriae felterrae glycosides IA, must not be less than 4.68mg.

16. the method for quality control of pharmaceutical composition as claimed in claim 15 is characterized in that comprising in this method following content assaying method:

It is an amount of that precision takes by weighing Radix Picriae felterrae glycosides IA reference substance, adds methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Get 2.22 times of amounts of this pharmaceutical composition day taking dose, the accurate title, decided porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 45 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate as need testing solution, promptly; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and calculate, and take amount of formulation this pharmaceutical composition day and contain Radix Picriae felterrae in Radix Picriae felterrae glycosides IA, must not be less than 4.68mg.

17. the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that comprising in this method in the following discrimination method one or more:

18. method of quality control as claimed in claim 17 is characterized in that comprising in this method in the following discrimination method one or more:

19. the method for quality control of pharmaceutical composition as claimed in claim 3 is characterized in that comprising in this method following content assaying method:

20. the method for quality control of pharmaceutical composition as claimed in claim 19 is characterized in that comprising in this method following content assaying method:

21. as claim 1,2,4, the application of 5 or 6 described pharmaceutical compositions in the medicine of preparation treatment chronic pelvic inflammatory disease.

22. have application in the medicine of antiinflammatory action, refrigeration function, itching-relieving action, analgesic activity, antibacterial action, the effect of expansion blood capillary or microcirculation improvement effect in preparation as claim 1,2,4,5 or 6 described pharmaceutical compositions.

23. the application of pharmaceutical composition as claimed in claim 3 in the medicine of preparation treatment chronic pelvic inflammatory disease.

24. pharmaceutical composition as claimed in claim 3 has application in the medicine of antiinflammatory action, refrigeration function, itching-relieving action, analgesic activity, antibacterial action, the effect of expansion blood capillary or microcirculation improvement effect in preparation.